Method of filling small vessels



States Mill Hill) OF FILLING MALL VESSELS Helmut Friedhofi, Koin-Raderthal, Germany, assignor to Firma Waither & Cie. Aittiengesellschaft, Kain-Dellbrucir, Germany N Drawing. Application dune 5, 1958 Serial No. 739,974

The present invention relates to a method of filling small vessels, and more particularly it relates to a method of producing a temperature responsive device, consisting essentially of a closed vessel filled with a liquid adapted to exert upon being subjected to a predetermined elevated temperature, a pressure against the inner wall of said vessel sufiicient to cause bursting of the same.

In fire detection and fire extinguishing devices such as sprinkler installations, it is frequently desirable to use as actuating device a small vessel which will burst upon being subjected to a predetermined elevated temperature, and which upon bursting will actuate signal devices, fire extinguishing devices or other devices useful for the intended purpose.

Such preferably small vessels which will burst upon being subjected to a predetermined elevated temperature,

are filled with a suitable liquid which by its expansion will cause the bursting of the vessel. conventionally, such vessels are filled with a suitable liquid by being evacuated in a bath of the liquid with which the vessel is to be filled and allowing the liquid to enter into the evacuated vessel under the influence of the atmospheric pressure to which the bath is exposed. In order to retain in the vessel a quantity of the liquid which will cause bursting of the vessel at the desired elevated temperature, the vessel-after being filled with the liquid and before being closed-is heated to another predetermined temperature so that a portion of the liquid within the vessel will be expelled due to the expansion of the liquid. The vessel which now contains as closely as possible the desired quantity of liquid is then closed by melting together the side walls of the capillary opening in the same. In order to obtain in this manner a device which will be responsive to relatively high temperatures, i. e., which will burst only upon being subjected to such relatively high temperature, it is necessary to use for the filling of the vessel a liquid having a high boiling point. Liquids which are suitable for this purpose, however, cannot be introduced into the vessel in the above described manner in such a way that the quantity of liquid remaining in the vessel can be controlled with sufficient accuracy to achieve reliable responsiveness of the device within a very small range of elevated temperature. In other words, it is not possible in the above described manner to produce'a temperature responsive device which will burst at exactly the desired temperature or within a narrow temperature range including the desired elevated bursting temperature.

It is therefore an object of the present invention to overcome the above described difiiculties in producing a temperature responsive device of the type described which will respond accurately within a narrow range of elevated temperature.

it is a further object of the present invention to provide a method forproducing a temperature responsive device of the type described, which can be carried out in a simple, accurate and economical manner.

It is another object of the present inventionto provide atent ice a method of introducing a liquid through a capillary opening into a vessel which is otherwise closed so as to substantially completely, or to any desired extent, fill the vessel with the liquid.

It is yet another and more specific object of the present invention to provide a temperature responsive device particularly for use in fire detection and fire fighting, which essentially consists of a small closed vessei filled with glycerine or with another liquid which at the desired predetermined temperature will exert such pressure on the walls of the vessel that the latter will burst.

Other objects and advantages of the present invention will become apparent from a further reading of the, description and the appendedclaims.

With the above and other objects in view, a method characteristic of the present invention may be described as a method of introducing a first liquid into a closed vessel formed with an opening of small cross section, so as to fill at least a substantial portion of the vessel with the first liquid, comprising the steps of introducing a small quantity of an auxiliary liquid into the vessel so as to fill a small portion only of the vessel with the auxiliary liquid, the auxiliary liquid having a boiling point below the boiling pointof the first liquid and being soluble in the first liquid, immersing the vessel containing the small quantity of the auxiliary liquid in a bath of the first liquid, subjecting the vessel containing the small quantity of the auxiliary liquid in the bath to a temperature above the boiling point of the auxiliary liquid and below the boiling point of the first liquid so as to evaporize the auxiliary liquid in the vessel, and cooling the bath of first liquid to below the boiling point of the auxiliary liquid, whereby the vapors of auxiliary liquid within the vessel immersed in said bath will be at least partially condensed, thus creating a partial vacuum within the vessel causing passage of first liquid from the bath through the small opening into the vessel, whereby auxiliary liquid originally introduced into the vessel will be dissolved in the first liquid and the same will fill at least a substantial portion of the vessel.

According to the present invention, a method of producing a temperature responsive device which consists essentially of a closed vessel adapted to burst upon being subjected to a predetermined degree of inner pressure, and of a liquid which substantially fills this vessel and which liquid is adapted to expand when subjected to the predetermined elevated temperature, so as to subject the vessel to the degree of inner pressure required for causing bursting of the vessel, may comprise the steps of introducing an auxiliary liquid into a vessel adapted to burst upon being subjected to the predetermined degree of inner pressure and being formed with a capillary opening, so as to fill a small portion only of the vessel with the auxiliary liquid, the auxiliary liquid having a boiling point below the boiling point of a first liquid adapted to expand upon being subjected to the predetermined elevated temperature so as to create the predetermined degree of pressure and being soluble in the first liquid, immersing the vessel containing the small quantity of the auxiliary liquid in a bath of the first liquid, subjecting the vessel containing the small quantity of the auxiliary liquid in the bath to a temperature above the boiling point of the auxiliary liquid and below the boiling point of the first liquid, so as to evaporize the auxiliary liquid in the vessel, cooling the bath of first liquid to below the boiling point of the auxiliary liquid, whereby the vapors of auxiliary liquid within the vessel will be condensed at least partially, thus creating a partial vacuum within the vessel causing passage of first liquid from the bath through the capillary opening into the vessel, whereby auxiliary liquid originally introduced into the vessel will be dissolved in the first liquid and the same will fill at least substantially the vessel, and closing the capillary opening of the vessel, thereby forming a closed vessel substantially filled with the first liquid which upon being subjected to the predetermined elevated temperature will create an overpressure suflicient to cause bursting of the vessel. 7

Thus, according to the present invention, into the pressure sensitive, preferably small, vessel, which advantageously might be made of glass, is first introduced a small quantity of an auxiliary liquid which is capable of being absorbed or dissolved in liquid or gaseous form by the temperature sensitive liquid with whichthe vessel is to be filled. Only a very small quantity of this auxiliary liquid is introduced into the vessel, the quantity, however, being suflicient to form upon evaporation a gas or vapor volume at least equal to the inner volume of the glass vessel or the like. I

The thusprepared vessel, i. e., the vessel containing a small quantity of the auxiliary liquid is then submerged underneath the surface of a bath consisting of the temperature sensitive liquid with which the vessel is to be filled. This liquid bath is preferably heated prior to immersion of the vessel into the same, to a temperature above the boiling point of the auxiliary liquid. While it would also be possible to heat the bath after the vessel has been submerged into the same, and while this later procedure also is to be considered within the scope of the present invention, it is preferred to pre-heat the bath to a temperature above the boiling point of the auxiliary liquid and thereafter to submerge the vessel containing a small quantity of the auxiliary liquid in the thus preheated bath. Thereby, the auxiliary liquid being subjected to the temperature of the bath which is higher than the boiling temperature of the auxiliary liquid, will immediately-evaporate; and the portion of the thus-formed vapors which exceeds the inner volume of the glass vessel will pass outwardly therefrom through the capillary opening of the same. When thereafter the temperature of the bath is reduced below the boiling temperature of the auxiliary'liquid, a portion of the vapors within the glass vessel will condense and due to the partial vacuum thus created Within the vessel, bath liquid will be drawn through the capillary opening into the vessel. Since, as stated above, the liquid of the bath is capable of absorbing or mixing with the vapors and with the liquid in the glass vessel, the partial vacuum therein will be increased and consequently additional bath liquid will be drawn through the capillary into the vessel until the same is substantially completely filled with the bath liquid which has absorbed the auxiliary liquid and its vapors which were contained within the vessel.

Thereafter, the temperature of the bath liquid is further reduced until the vessel submerged therein is cooled to the dosing temperature. The vessel is then removed from the bath and further cooled, whereby it is achieved due to contraction of the liquid within the vessel upon such further cooling that a predetermined amount of air enters the vessel. Thereafter the capillary opening of the vessel is closed by melting.

In the case of a glass vessel of a customary size which will have an inner volume of about 80 cubic millimeters, it will be sufficient when about 2 cubic millimeters of the auxiliary liquid are sucked into the vessel, i. e., the quantity of auxiliary liquid within the vessel is equal to about. 2.5 percent of the inner volume of the vessel. Upon evaporation of the auxiliary liquid, the volume of the same will be increased, for instance in the case of water to about 800 times the volume of the originally introduced liquid, or to about 1,600 cubic millimeters. The volume of the thus-formed vapors is thus equal to about times the inner volume of the vessel. By forming this relatively very large quantity of vapors, the mag'or portion of which escapes through the capillary opening of the vessel, the air remaining in the vessel after introduction of the two cubic millimeters of auxiliary liquid all) which amounts to about 78 cubic millimeters will for all practical purposes be completely removed from the vessel so that the same contains now only the vapors formed by evaporation of the auxiliary liquid. If for instance, in accordance with the preferred manner of carrying out the present invention, water is used as auxiliary liquid and water-free glycerine having a boiling point of 290 as the liquid with which the vessel is to be filled, it is possible in this manner to produce a temperature responsive device of great accuracy which will always burst at substantially the same elevated temperature.

The following example of a preferred way of carrying out the method of the present invention is given as illus trative only, the invention however not being limited to the Specific details of the example.

EXAMPLE l A glass vessel having a capillary opening and a volume of about 80' cubic millimeters as described above, is taken from-stock at room temperature of for instance about 20 C. Assuming that the room temperature is about 20 C., the vessel which is filled with air is then heated for a short period of time at 40 C., so that the air within the vessel will expand and a small portion of the air will pass from the interior of the vessel through the capillary opening. Thereafter, the thus-heated glass vessel is submerged in water of 20 C. Water would not enter into the completely air-filled vessel in View of the small diameter of the capillary opening. However, due to cooling the vessel and the air therein from 40 C. to about 20 C., the volume of the air in the vessel is reduced and a small quantity of water, approximately 2 cubic millimeters will enter into the vessel through the capillary opening of the same. Thereafter, the glass vessel is removed from the water bath, its outside is dried and the vessel thereafter submerged in a bath of glycerine having a temperature of between 130 C. and 140 C. Upon submersion in the hot glycerine, the water within the vessel will quickly evaporate and due to the overpressure formed thereby within the vessel, excess vapor will be driven out together with the remainder of the air within the glass vessel. Upon subsequent cooling of the glycerine bath-by about 20 C. to a temperature of about between. C. and C., the water vapor volume within the vessel will be reduced and thus a small quantity of glycerine will be sucked through the capillary opening into the vessel. The glycerine which thus enters the vessel will immediately absorb the water vapors remaining in the same, thereby, reducing the pressure within the vessel so that additional glycerine is sucked into the vessel until the same is substantially completely filled with glycerine. Thereafter, the glycerine bath is cooled to the dosing temperature which is a temperature of about 20 below the temperature at which the filled vessel is supposed to burst. The vessel which is now completely filled with glycerine at the dosing temperature, is now removed from the glycerine bath.

It is possible at this point to immediately melt down the capillary with a hot flame and thus to close the vessel. However, according to a preferred embodiment of the present invention, the vessel is first cooled to room temperature and only after thus cooling the vessel and cleaning the outside of the same of the glycerine adhering thereto, the capillary is closed. During cooling of the glycerine-filled vessel from the dosing temperature which, for instance may be 80 C. if it is desired that the vessel should burst at 100 (3., down to room temperature of for instance 20 C., the glycerine volume within the vessel is reduced. Thus, a small quantity of air will enter through the capillary and form a small air bubble underneath the capillary opening. This has the advantage that the melting down of the capillary so as to close the vessel can be carried out with certainty and will not be made ditficult due to the presence of glycerine which may flow from the capillary due to the heating of the same with the glass blowers flame. The presence of glycerine at the outside of the capillary during the melting down of the same can greatly effect the pressure resistance of the vessel, thus interfering with the temperature responsiveness of the device. This is one of the reasons why conventional glass vessels of this kind possess a greatly varying resistance against inner over-pressure which may vary between 200 and 400 atmospheres, and which varies at the average between about 270 and 320 atmospheres. Due to the fact that according to the described preferred method, the vessel is closed by melting down the capillary at room temperature and so that a small air bubble is retained in the interior of the vessel, it is possible to check the pressure resistance of the completed vessel, for instance by heating the closed vessels with hot air to about 80 C. The vessels which possess insufiicient pressure resistance will burst thereby and will thus be removed, while such vessels which possess abnormally high pressure resistance would still burst upon an only insignificant increase of the temperature over the desired temperature. Such increase in temperature required for causing bursting of glass vessels possessing abnormally high pressure resistance will be within the range of only about two or three degrees centigrade.

Furthermore, it is possible by comparing the size of the air bubbles in the closed vessels, to exclude from any one series of vessels which are supposed to have an identical bursting temperature, those vessels which show an air bubble greater than desired so that the then remaining vessels will burst within an extremely narrow temperature range.

As described in the foregoing example, the liquid which is filled into the vessel in order to cause bursting of the same at a predetermined elevated temperature, is glycerine, and water is used as the auxiliary liquid which is evaporized and which is miscible with glycerine. However, it is also'within the scope of the present invention to use as auxiliary liquid and as filling liquid any other liquids which possess the desired qualities, namely that the boiling point of the auxiliary liquid is lower than the boiling point of the liquid with which the vessel is eventually to be filled, that the two liquids are soluble in each other, i. e., that the filling liquid is capable of absorbing the vapors of the auxiliary liquid, and that the temperature expansion co-eflicient of the filling liquid is such that the desired over-pressure can be produced at the predetermined elevated temperature at which the vessel is supposed to burst. Glycerine as filling liquid in combination with water as the auxiliary liquid gives excellent results, since with these two liquids pressure vessels can be produced which will burst at any desired temperature within the range of between 70 C. and 270 C., which range is sufficient for most practical applications.

The following table lists several combinations of filling liquids and auxiliary liquids which may be used advantageously according to the present invention, the invention however not being limited to the specific liquids listed below.

Without further analysis, the foregoing will so fully reveal the gist of the present invention that others can by applying current knowledge readily adapt it for various applications without omitting features that, from the standpoint of prior art, fairly constitute essential characteristics of the generic or specific aspects of this invention and, therefore, such adaptations should and are intended to be comprehended within the meaning and range of equivalence of the following claims.

What is claimed as new and desired to be secured by Letters Patent is:

1. A method of introducing a first liquid into a closed vessel formed with an opening of small cross section, so as to fill at least a substantial portion of said vessel with said first liquid, comprising the steps of introducing a small quantity of an auxiliary liquid into said vessel so as to fill a small portion only of said vessel with said auxiliary liquid, said auxiliary liquid having a boiling point below the boiling point of said first liquid and being soluble in said first liquid; immersing said vessel containing said small quantity of said auxiliary liquid in a bath of said first liquid; subjecting said vessel containing said small quantity of saidauxiliary liquid in said bath to a temperature above the boiling point of said auxiliary liquid and below the boiling point of said first liquid, so as to evaporize said auxiliary liquid in said vessel; and cooling said bath of first liquid to below the boiling point of said auxiliary liquid, whereby the vapors of auxiliary liquid within said vessel immersed in said bath will be condensed at least partially, thus creating a partial vacuum within said vessel causing passage of first liquid from said bath through said small opening into said vessel, whereby auxiliary liquid originally introduced into said vessel will be dissolved in said first liquid and the same will fill at least a substantial portion of said vessel.

2. A method of introducing a first liquid into a closed vessel formed with a capillary opening, so as to fill at least a substantial portion or" said vessel with said first liquid, comprising the steps of introducing a small quantity of an auxiliary liquid into said vessel so as to fill a small portion only of said vessel with said auxiliary liquid, said auxiliary liquid having a boiling point below the boiling point of said first liquid and being soluble in said first liquid; immersing said vessel containing said small quantity of said auxiliary liquid in a bath of said first liquid; subjecting said vessel containing said small quantity of said auxiliary liquid in said bath to a temperature above the boiling point of said auxiliary liquid and below the boiling point of said first liquid, so as to evaporize said auxiliary liquid in said vessel; and cooling said bath of first liquid to below the boiling point of said auxiliary liquid, whereby the vapors of auxiliary liquid within said vessel immersed in said bath will be condensed at least partially, thus creating a partial vacuum within said vessel causing passage of first liquid from said bath through said capillary opening into said vessel, whereby auxiliary liquid originally introduced into said vessel will be dissolved in said first liquid and the same will fill at least a substantial portion of said vessel.

3. A method of introducing a first liquid into a closed vessel formed with a capillary opening, so as to fill at least a substantial portion of said vessel with said first liquid, comprising the steps of introducing a small quantity of an auxiliary liquid into said vessel so as to fill a small portion only of said vessel with said auxiliary liquid, said auxiliary liquid having a boiling point below the boiling point of said first liquid and being soluble in said first liquid; immersing said vessel containing said small quantity of said auxiliary liquid in a bath of said first liquid having a temperature above the boiling point of said auxiliary liquid and below the boiling point of said first liquid, so as to evaporize said auxiliary liquid in said vessel; and cooling said bath of first liquid to below the boiling point of said auxiliary liquid, whereby the vapors of auxiliary liquid within said vessel immersed in said bath will be condensed at least partially, thus creating a partial vacuum within said vessel causing passage of first liquid from said bath through said capillary openinginto said vessel, whereby auxiliary liquid originally introduced into said vessel will be dissolved in said first liquid and the same will fill at least a substantial portion of said vessel.

4. A method of introducing a first liquid into a closed vessel formed with'a capillary opening, so as to fill at least a substantial portion of said vessel with said first liquid, comprising the steps of introducing a small quantity of an auxiliary liquid into said vessel so as to fill a small portion only of said vessel with said auxiliary liquid, said auxiliary liquid having a boiling point below the boiling point of said first liquid and being soluble in said first liquid; immersing said vessel containing said small quantity of said auxiliary liquid in a bath of said first liquid; heating said bath to a temperature above the boiling point of said auxiliary liquid and below the boiling point of said first liquid, so as to evaporize said auxiliary liquid in said vessel; and cooling said bath of first liquid to below the boiling point of said auxiliary liquid, whereby the vapors of auxiliary liquid within said vessel immersed in said bath will be condensed at least partially, thus creating a partial vacuum within said vessel causing passage of first liquid from said bath through said capillary opening into said vessel, whereby auxiliary liquid originally introduced into said vessel will be dissolved in said first liquid and the same will fill at least a substantial portion of said vessel.

5. A method of introducing a first liquid selected from the group consisting of glycol and glycerine into a closed vessel formed with a capillary opening, so as to fill at least a substantial portion of said vessel with said first liquid, comprising the steps of introducing a small quantity of water into said vessel so as to fill a small portion only of said vessel with said Water; immersing said vessel containing said small quantity of water in a bath of said first liquid; subjecting said vessel containing saidsmall quantity of water in said bath to a temperature above the boiling point of water and below the boiling point of said first liquid, so as to evaporize said water in said vessel; and cooling said bath of first liquid to below the boiling point of Water, whereby the water varors within said vessel immersed in said bath will be condensed at least partially, thus creating a partial vacuum within said vessel causing passage of first liquid from said bath through said capillary opening into said vessel, whereby water originally introduced into said vessel will be dissolved in said first liquid and the same Will fill at least a substantial portion of said vessel.

6. A method of introducing glycetine into a closed vessel formed with a capillary opening, so as to fill at least a substantial portion of said vessel with said glycerine, comprising the steps of introducing a small quantity of water into said vessel so as to fill a small portion only of said vessel with said water; immersing said vessel containing said small quantity of water in a bath of glycerine; subjecting said vessel containing said small quantity of water in said bath of glycerine to a temperature above the boiling point of water and below the boiling point of glycerine, so as to evaporize said water in said vessel; and cooling said bath of glycerine to below the boiling point of water, whereby the water vapors within said vessel immersed in said bath will be condensed at least partially, thus creating a partial vacuum within said vessel causing passage of glycerine from said bath through said capillary opening into said vessel, whereby water originally introduced into said vessel will be dissolved in said glyceriue and the same will fill at least a substantial portion of said vessel.

7. A method of introducing a first liquid into a closed vessel formed with a capillary opening, so as to fill at least a substantial portion of said vessel with said first liquid, comprising the steps of heatingsaid vessel to a first temperature being somewhat higher than a second predetermined temperature; submerging the thus heated vessel into a bath or an auxiliary liquid maintained at said second predetermined temperature, thereby cooling said vessel and somewhat reducing the volume of air within the same thus creating a partial vacuum within said vessel causing introduction into the same through the capillary opening thereof of a small quantity of said auxiliary liquid, the temperature differential between said first temperature and said second predetermined temperature being so chosen that upon cooling of said vessel in said bath, the quantity of auxiliary liquid sucked into said vessel will be sutficiently large to form upon heating above its boiling point a quantity of vapors of said auxiliary liquid being sufiicient to completely fill said vessel, said auxiliary liquid having a boiling point below the boiling point of said first liquid and being soluble in said first liquid; immersing said vessel containing said small quantity of said auxiliary liquid in a bath or" said first liquid; subjecting said vessel containing said small quantity of said auxiliary liquid in said bath to a temperature above the boiling point of said auxiliary liquid and below the boiling point of said first liquid, so as to evaporize said auxiliary liquid in said vessel; and cooling said bath of first liquid to below the boiling point of said auxiliary liquid, whereby the vapors of auxiliary liquid within said vessel immersed in said bath will be condensed at least partially, thus creating a partial vacuum within said vessel causing passage of first liquid from said bath through said capillary opening into said vessel, whereby auxiliary liquid originally introduced into said vessel will be dissolved in said first liquid and the same will fill at least a substantial portion of said vessel.

8. A method of producing a temperature responsive device, consisting essentially of a closed vessel adapted to burst upon being subjected to a predetermined degree of inner pressure, and of a liquid substantially filling said vessel, said liquid being adapted to expand, upon being subjected to a predetermined elevated temperature, so as to subject said vessel to said predetermined degree of inner pressure, comprising the steps of introducing an auxiliary liquid into a vessel adapted to burst upon being subjected to said predetermined degree of inner pressure and being formed with a capillary opening, so as to fill a small portion only of said vessel with said auxiliary liquid, said auxiliary liquid having a boiling point below the boiling point of a first liquid adapted to expand upon being subjected to said predetermined elevated temperature so as to create said predetermined degree of pressure and being soluble in said first liquid; immersing said vessel containing said small quantity of said auxiliary liquid in a bath of said first liquid; subjecting said vessel containing said small quantity of said auxiliary liquid in said bath to a temperature above the boiling point of said auxiliary liquid and below the boiling point of said first liquid, so as to evaporize said auxiliary liquid in said vessel; cooling said bath of first liquid to below the boiling point of said auxiliary liquid, whereby the vapors of auxiliary liquid within said vessel immersed in said bath will be condensed at least partially, thus creating a partial vacuum within said vessel causing passage of first liquid from said bath through said capillary opening into said vessel, whereby auxiliary liquid originally introduced into said vessel will be dissolved in said first liquid and the same will at least substantially fill said vessel; and closing said capillary opening of said vessel, thereby forming a closed vessel substantially filled with said first liquid which upon being subjected to said predetermined elevated temperature will create an overpressure suflicient to cause bursting of said vessel.

9. A method of filling a small vessel formedwith a capillary opening, such as a vessel to be used after closing of the opening as a temperature-sensitive vessel adapted to burst at a predetermined elevated temperature, comprising the steps of introducing into said vessel a quantity of an auxiliary liquid said quantity being small relative to the inner volume of said vessel; submerging said vessel with said small quantity of said auxiliary liquid therein into a bath of a filling liquid to be filled into said vessel, said filling liquid having a boiling temperature higher than the boiling temperature of said auxiliary liquid and being miscible with the same, the temperature of said bath being above the boiling temperature of said auxiliary liquid and below the boiling temperature of said filling liquid; cooling said bath to a temperature below the boiling temperature of said auxiliary liquid and also below the predetermined elevated temperature at which said temperature-sensitive vessel is adapted to burst, whereby upon submersion of said vessel in said bath, the auxiliary liquid within the vessel is evaporated and excess vapor escapes through the capillary opening of said vessel, and upon cooling of said vessel Within said bath said filling liquid is sucked into said vessel through said capillary opening, absorbing the vapor of said auxiliary liquid within said vessel, so that said vessel is substantially completely filled with said filling liquid; removing the thus filled vessel from said bath; and closing the capillary opening of the same.

10. A method of introducing a first liquid into a closed vessel formed with a capillary opening, so as to fill at least a substantial portion of said vessel with said first liquid, comprising the steps of introducing a small quantity of an auxiliary liquid into said vessel so as to fill a small portion only of said vessel with said auxiliary liquid, said auxiliary liquid having a boiling point below the boiling point of said first liquid and being soluble in said first liquid; immersing said vessel containing said small quantity-of said auxiliary liquid in a bath of said first liquid; subjecting said vessel containing said small quantity of said auxiliary liquid in said bath to a temperature above the boiling point of said auxiliary liquid and below the boiling point of said first liquid, so as to evaporize said auxiliary liquid in said vessel; and cooling said bath of first liquid to below the boiling point of said auxiliary liquid, whereby the vapors of auxiliary liquid within said vessel immersed in said bath will be condensed at least partially, thus creating a partial vacuum within said vessel causing passage of first liquid from said bath through said capillary opening into said vessel, whereby the vapor of auxiliary liquid within said vessel will be dissolved in said first liquid so that the same will substantially completely fill said vessel; removing the thus filled vessel from said bath; further cooling said vessel so as to contract the volume of said first liquid within said vessel and thus causing introduction of a small quantity of air through said capillary opening into said vessel; and closing said capillary opening.

No references cited. 

